CN110165171B - In-situ self-assembly nano flower-shaped cobalt disulfide/rGO composite material and preparation method and application thereof - Google Patents
In-situ self-assembly nano flower-shaped cobalt disulfide/rGO composite material and preparation method and application thereof Download PDFInfo
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- CN110165171B CN110165171B CN201910410113.1A CN201910410113A CN110165171B CN 110165171 B CN110165171 B CN 110165171B CN 201910410113 A CN201910410113 A CN 201910410113A CN 110165171 B CN110165171 B CN 110165171B
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Abstract
The invention discloses an in-situ self-assembly nanometer flower-shaped cobalt disulfide/rGO composite material and a preparation method and application thereof, wherein the in-situ self-assembly nanometer flower-shaped cobalt disulfide/rGO composite material is prepared by adding a GO aqueous solution into a mixed solution of a soluble cobalt salt aqueous solution and a vulcanizing agent aqueous solution, stirring and carrying out ultrasonic treatment, reacting the obtained GO mixed solution in a stainless steel reaction kettle at 150-280 ℃, cooling along with a furnace, carrying out suction filtration, and carrying out freeze drying treatment on the obtained solid. The composite material has a three-dimensional microstructure in a nanometer flower shape, wherein the nanometer flower is composed of a cobalt disulfide single crystal wafer, the nanometer flower grows on a two-dimensional rGO nanometer sheet substrate in situ, the substrate can effectively accommodate the volume effect of the cobalt disulfide in the charging and discharging process, and the conductivity is good. Meanwhile, the composite material has excellent charge-discharge cycle performance and rate capability, and can be applied to the field of lithium ion battery cathode materials.
Description
Technical Field
The invention belongs to the technical field of lithium ion battery cathode materials, and particularly relates to an in-situ self-assembled nano flower-shaped cobalt disulfide/rGO composite material and a preparation method and application thereof.
Background
Along with the progress and development of society, the energy problem faced by human is increasingly prominent. Lithium ion batteries, as the most successful commercial energy storage devices at present, have relieved some of the concerns of people about energy storage, and are therefore popular among people in all fields. In particular, lithium ion batteries are widely developed and applied in the field of electric vehicles due to their advantages of green/environmental protection, recyclability, and the like. At present, the negative active materials adopted in the lithium ion batteries in the market are various graphite materials with good electrical conductivity/layered structures, the theoretical specific capacity of the negative active materials is 372mAh/g, the negative active materials are relatively suitable for the intercalation and deintercalation of lithium ions, and the negative active materials show higher first coulombic efficiency and better cycling stability. However, with the development of industry and technology, people have raised higher requirements on performance parameters of lithium ion batteries, such as capacity, energy density and cycle life, and lithium ion batteries prepared from graphite cathode materials cannot meet the requirements of high-specific-energy lithium ion batteries at present.
The cobalt disulfide is used as the lithium ion battery electrode material, the theoretical specific capacity of the cobalt disulfide is usually as high as more than 700mAh/g, which is at least two times of that of the commercial graphite cathode material, in addition, the sulfur element storage capacity is very rich, the price is very low, and the lithium embedding voltage of the cobalt disulfide material is relatively low, so that the cobalt disulfide material is very suitable for being used as the cathode material of the next generation of high-energy lithium ion battery cell. However, in the process of charging and discharging lithium ions, the material generates a large volume expansion rate, which causes pulverization and falling of the cobalt disulfide material, and on one hand, the contact between the active material and the current collector is influenced, and the hindered electron transmission process is influenced; on the other hand, the solid electrolyte interface film is gradually thickened in the circulation process, so that lithium ions are continuously consumed, the internal impedance of the battery is increased, the capacity and the coulombic efficiency are continuously reduced, and the circulation life is reduced. Therefore, it is necessary to buffer the volume effect generated during the charge and discharge processes thereof, thereby improving the cycle stability thereof as much as possible.
In view of the above problems, the currently common solutions are to prepare cobalt sulfide nanoparticles, prepare cobalt sulfide sheets, and compound them with carbon materials, which is a promising method. However, the existing cobalt sulfide/graphene composite material only carries out simple mechanical coating on the cobalt disulfide material, and has limited improvement on capacity exertion and cycle life, and cannot meet the current industrialized demand. rGO is a two-dimensional material with excellent performance, and its excellent conductivity and nano-layered structure are favored by scientists in various fields. However, the special value of the novel lithium ion composite material is not fully realized in the preparation of the novel lithium ion composite material. Particularly, no research report exists at present, and the lithium ion composite material with the cobalt disulfide nano flower-shaped three-dimensional structure grows in situ on the two-dimensional rGO nano sheet.
Disclosure of Invention
In order to overcome the defects and shortcomings of the carbon negative electrode material and the similar composite material in the application of the high-energy-density lithium ion battery in the prior art, the invention mainly aims to provide the in-situ self-assembled nano flower-shaped cobalt disulfide/rGO composite material. The composite material has a good three-dimensional nano flower-shaped flexible structure, can fully exert the capacity of the cobalt disulfide nano particles, can effectively accommodate the volume effect of the cobalt disulfide nano particles in the charge and discharge processes, and has good conductivity, excellent multiplying power and cycle performance.
The invention also aims to provide a preparation method of the in-situ self-assembly nano flower-shaped cobalt disulfide/rGO composite material.
The invention further aims to provide application of the in-situ self-assembled nano flower-shaped cobalt disulfide/rGO composite material.
The purpose of the invention is realized by the following technical scheme:
the in-situ self-assembly nanometer flower-shaped cobalt disulfide/rGO composite material is prepared by adding a GO aqueous solution into a mixed solution of a soluble cobalt salt aqueous solution and a vulcanizing agent aqueous solution, reacting the obtained GO mixed solution in a stainless steel reaction kettle at 150-280 ℃ after stirring and ultrasonic treatment, cooling along with a furnace, and performing freeze drying treatment on the obtained solid after suction filtration.
Preferably, the soluble cobalt salt in the soluble cobalt salt aqueous solution is CoCl2、C4H6CoO4、CoSO4、Co(NO3)2And hydrates of one or more of the above salts.
Preferably, the vulcanizing agent in the vulcanizing agent aqueous solution is more than one of sodium sulfide, thioacetamide and L-cysteine.
Preferably, the molar ratio of the soluble cobalt salt to the vulcanizing agent is (0.5-1): 1.
preferably, the mass ratio of the rGO to the vulcanizing agent is (0.1-1): 1.
preferably, the concentration of the soluble cobalt salt aqueous solution is 0.01-0.1 mol/L, and the concentration of the vulcanizing agent aqueous solution is 0.01-0.1 mol/L.
Preferably, the stirring time is 5-60 min; the ultrasonic time is 30-120 min, and the reaction time is 12-36 h; the temperature of the freeze drying is-40 to-50 ℃, and the time of the freeze drying is 24 to 48 hours.
The preparation method of the in-situ self-assembly nano flower-shaped cobalt disulfide/rGO composite material comprises the following specific steps:
s1, respectively dissolving soluble cobalt salt and a vulcanizing agent in deionized water to obtain a solution A and a solution B;
s2, adding the solution A into the solution B, and mixing and stirring uniformly to obtain a solution C;
s3, adding the GO aqueous solution into the solution C, stirring, and performing ultrasonic dispersion to obtain a GO mixed solution D;
s4, pouring the solution D into a stainless steel reaction kettle, drying, preserving heat, cooling along with a furnace, and then performing suction filtration to obtain a solid D;
and S5, carrying out freeze drying on the solid D to obtain the in-situ self-assembled nano flower-shaped cobalt disulfide/rGO composite material.
Preferably, in the step S1, the ratio of the mass of the soluble cobalt salt to the volume of the deionized water is (1000-2000): 100 mg/mL; the mass ratio of the vulcanizing agent to the deionized water is (40-400): 100 mg/mL.
The in-situ self-assembled nano flower-shaped cobalt disulfide/rGO composite material is applied to the field of lithium ion battery cathode materials.
The method comprises the steps of dissolving soluble cobalt salt and a vulcanizing agent in deionized water respectively, then fully mixing and completely reacting the soluble cobalt salt and the vulcanizing agent, then adding a GO aqueous solution, adsorbing a product obtained after reaction on a GO two-dimensional nano sheet, uniformly dispersing and stirring, then carrying out simple hydrothermal reaction to enable cobalt disulfide to grow into a single crystal sheet on the GO nano sheet in situ, then carrying out self-assembly to form a nanoflower structure, enabling the cobalt disulfide and a GO material to be combined very tightly on a microstructure, simultaneously reducing GO into rGO, and forming an ordered and interconnected porous sheet layer structure between sheets. And finally, carrying out suction filtration and freeze drying treatment on the product to obtain the three-dimensional nano flower-shaped cobalt disulfide/rGO composite material. In the cathode material obtained by the technical scheme, the cobalt disulfide single crystal wafer is self-assembled on the rGO sheet to form a three-dimensional nanoflower structure, and meanwhile, the rGO sheet and the sheets are also mutually connected to form an ordered porous structure, so that the three-dimensional nanoflower three-dimensional porous structure is finally obtained.
The cobalt disulfide in the in-situ self-assembly nanometer flower-shaped cobalt disulfide/rGO composite material is in a nanometer flower shape, so that gram capacity exertion of the material in the charging and discharging process is favorably improved, and the nanometer flower is composed of nanometer single crystal wafers, is single and stable in structure and shows good cycling stability. Meanwhile, the nanoflower is self-assembled on the rGO nano-sheet in situ, so that the contact resistance between the nanoflower and the rGO nano-sheet can be reduced. And ordered interconnected porous channels formed among the rGO nano sheets are beneficial to the storage of lithium ions and the permeation of electrolyte, so that the cobalt disulfide nano flowers are better contacted with the electrolyte. In addition, the cobalt disulfide nanoflower of in situ growth has played the supporting role to the rGO layer, is favorable to preventing the collapse of lamellar structure and the restack of rGO layer, keeps better flexible construction, provides effectual passageway for electron and lithium ion's transmission for cobalt disulfide nanoflower/rGO combined material has better rate capability. And the rGO layer positioned outside the cobalt disulfide nanoflowers isolates the direct contact between the cobalt disulfide nanoflowers and electrolyte, so that the solid electrolyte interface film is ensured to be on the surface of the graphene, and a stable solid electrolyte interface film is formed. And the three-dimensional flexible rGO sheet can effectively accommodate the volume effect of cobalt disulfide in the charge and discharge process, and keep higher specific capacity. Therefore, the in-situ self-assembly nano flower-shaped cobalt disulfide/rGO composite material prepared by the technical scheme of the application has excellent charge-discharge cycle performance and rate capability.
Compared with the prior art, the invention has the following beneficial effects:
1. the in-situ self-assembly nano flower-shaped cobalt disulfide/rGO composite material has a good three-dimensional nano flower-shaped flexible structure, can fully play the capacity of cobalt disulfide nano particles, can effectively accommodate the volume effect of the cobalt disulfide nano particles in the charge and discharge processes, and has good conductivity, excellent multiplying power and cycle performance.
2. The active substance is cobalt disulfide, is in a nanoflower structure formed by self-assembly of single crystal nano, and is beneficial to full play of capacity removal and maintenance of excellent cycling stability in the charge-discharge cycling process. Meanwhile, the rGO enables the composite material to have a three-dimensional porous structure, so that ion storage and electrolyte permeation are facilitated, better contact between active substances and electrolyte is facilitated, an effective channel is provided for transmission of electrons and lithium ions, and the cobalt disulfide/rGO composite material has better rate capability.
3. Due to the supporting effect of the cobalt disulfide nanoflowers on the rGO, the high-performance cobalt disulfide nanoflowers can keep a good flexible structure, can effectively accommodate the volume effect of the cobalt disulfide in the charging and discharging processes, keeps high specific capacity and good conductivity, and has excellent charging and discharging cycle performance, rate capability and high first coulombic efficiency.
Drawings
FIG. 1 is a scanning electron microscope image of the in-situ self-assembled nano flower-like cobalt disulfide/rGO composite material prepared in example 1.
Fig. 2 is a rate charge and discharge performance curve of the in-situ self-assembled nano flower-like cobalt disulfide/rGO composite material prepared in example 1.
Detailed Description
The present invention will be described in further detail with reference to examples, but the embodiments of the present invention are not limited thereto.
Example 1
1. Adding 5mmol of CoSO4·7H2Dissolving O and 10mmol NaS in 40mL of deionized water respectively to obtain a pink A solution and a transparent B solution;
2. slowly adding the solution A into the solution B in the step 1, uniformly mixing, and fully stirring for 30min to obtain a light red solution C;
3. weighing an aqueous solution containing 50mg of GO, adding the aqueous solution into the solution C in the step 2, stirring for 30min, and performing ultrasonic dispersion for 10min to obtain a GO mixed solution D;
4. pouring the solution D obtained in the step 3 into a 100mL stainless steel reaction kettle, then placing the stainless steel reaction kettle into a forced air drying oven, preserving the heat for 36 hours at the temperature of 150 ℃, cooling along with the furnace, and then performing suction filtration to obtain a solid D;
5. and (4) drying the solid D in the step (4) in a freeze drying box to obtain the in-situ self-assembled nano flower-shaped cobalt disulfide/rGO composite material.
Fig. 1 is a scanning electron microscope picture of the in-situ self-assembled nano flower-like cobalt disulfide/rGO composite material prepared in the present embodiment. As can be seen from figure 1, the cobalt disulfide is in a nanometer flower shape with the size of about 200-300 nm, grows on the reduced graphene oxide sheet in situ, and is in a cross flower shape formed by nanometer sheets with the thickness of 20-30 nm. Fig. 2 is a rate charge and discharge performance curve of the in-situ self-assembled nano flower-like cobalt disulfide/rGO composite material prepared in the present embodiment. As can be seen from FIG. 2, the charge capacity and rate capability of pure cobalt disulfide are poor, while the cobalt disulfide/rGO composite material has excellent charge and discharge performance, the gram capacity can be kept at 500mAh/g under the current density of 2.0A/g, and after high-rate charge and discharge, the capacity can be recovered to 700mAh/g (0.5A/g), which indicates that the cobalt disulfide/rGO composite material has strong reversible recovery capability.
Example 2
1. 3mmol of CoCl2·6H2Dissolving O and 3mmol of TAA (thioacetamide) in 40mL of deionized water respectively to obtain a pink A solution and a transparent B solution;
2. slowly adding the solution A into the solution B in the step 1, uniformly mixing, and fully stirring for 30min to obtain a light red solution C;
3. weighing an aqueous solution containing 30mg of GO, adding the aqueous solution into the solution C in the step 2, stirring for 30min, and performing ultrasonic dispersion for 10min to obtain a GO mixed solution D;
4. pouring the solution D obtained in the step 3 into a 100mL stainless steel reaction kettle, then placing the stainless steel reaction kettle into a forced air drying oven, preserving the heat for 36 hours at the temperature of 150 ℃, cooling along with the furnace, and then performing suction filtration to obtain a solid D;
5. and (4) drying the solid D in the step (4) in a freeze drying box to obtain the in-situ self-assembled nano flower-shaped cobalt disulfide/rGO composite material.
Example 3
1. 4mmol of CoCl2·6H2Dissolving O and 4mmol L-cysteine in 40mL deionized water respectively to obtain pink A solution and transparent B solution;
2. slowly adding the solution A into the solution B in the step 1, uniformly mixing, and fully stirring for 30min to obtain a light red solution C;
3. weighing an aqueous solution containing 40mg of GO, adding the aqueous solution into the solution C in the step 2, stirring for 30min, and performing ultrasonic dispersion for 10min to obtain a GO mixed solution D;
4. pouring the solution D obtained in the step 3 into a 100mL stainless steel reaction kettle, then placing the stainless steel reaction kettle into a forced air drying oven, preserving the heat for 36 hours at the temperature of 150 ℃, cooling along with the furnace, and then performing suction filtration to obtain a solid D;
5. and (4) drying the solid D in the step (4) in a freeze drying box to obtain the in-situ self-assembled nano flower-shaped cobalt disulfide/rGO composite material.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations and simplifications are intended to be included in the scope of the present invention.
Claims (5)
1. The in-situ self-assembly nanometer flower-shaped cobalt disulfide/rGO composite material is characterized in that a GO aqueous solution is added into a mixed solution of a soluble cobalt salt aqueous solution and a vulcanizing agent aqueous solution, the mixed solution is stirred and subjected to ultrasonic treatment, the obtained GO mixed solution is reacted for 12-36 hours at 150-280 ℃ in a stainless steel reaction kettle, furnace cooling is carried out, and the obtained solid is subjected to freeze drying treatment after suction filtration to prepare the in-situ self-assembly nanometer flower-shaped cobalt disulfide/rGO composite material; the soluble cobalt salt and the vulcanizing agent in the mixed solution are respectively CoCl2And thioacetamide, CoCl2And L-cysteine, CoSO4And sodium sulfide; the molar ratio of the soluble cobalt salt to the vulcanizing agent is (0.5-1): 1; the mass ratio of the rGO to a vulcanizing agent is (0.1-1): 1.
2. the in-situ self-assembled nanoflower-shaped cobalt disulfide/rGO composite material according to claim 1, wherein the concentration of the soluble cobalt salt aqueous solution is 0.01-0.1 mol/L, and the concentration of the vulcanizing agent aqueous solution is 0.01-0.1 mol/L.
3. The in-situ self-assembled nano flower-like cobalt disulfide/rGO composite material according to claim 1, wherein the stirring time is 5-60 min; the ultrasonic time is 30-120 min, the freeze drying temperature is-40 to-50 ℃, and the freeze drying time is 24-48 h.
4. The preparation method of in-situ self-assembled nano flower-like cobalt disulfide/rGO composite material according to any one of claims 1-3, characterized by comprising the following specific steps:
s1, respectively dissolving soluble cobalt salt and a vulcanizing agent in deionized water to obtain a solution A and a solution B;
s2, adding the solution A into the solution B, and mixing and stirring uniformly to obtain a solution C;
s3, adding the GO aqueous solution into the solution C, stirring, and performing ultrasonic dispersion to obtain a solution D;
s4, pouring the solution D into a stainless steel reaction kettle, placing the stainless steel reaction kettle into a forced air drying box for heat preservation treatment, cooling along with a furnace, and then performing suction filtration to obtain a solid D;
and S5, freezing and drying the solid D to obtain the in-situ self-assembled nano flower-shaped cobalt disulfide/rGO composite material.
5. The use of the in situ self-assembled nanoflower-shaped cobalt disulfide/rGO composite material of any one of claims 1-3 in the field of lithium ion battery negative electrode materials.
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| CN111129494B (en) * | 2019-12-28 | 2021-09-10 | 常州大学 | Preparation method of sulfo-spinel/graphene electrode material and electrode material thereof |
| CN113120970B (en) * | 2021-03-26 | 2023-03-24 | 东南大学 | Method for preparing compound containing crystal water cobalt sulfate and redox graphene |
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